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Ceftezol drug intermediates 2-(1H-1-4 imidazolyl) acetic acid synthesis method

机译:头孢唑醇药物中间体2-(1H-1-4咪唑基)乙酸的合成方法

摘要

#$%^&*AU2016102314A420170223.pdf#####ABSTRACT Ceftezol drug intermediates 2-(1H-1-4 imidazolyl) acetic acid synthesis method, comprising the following steps: (I) a reaction vessel was added 0.51mol 2-(5-nitro-1H-1-tetrazolyl) acetic acid (2), 0.56-0.59mol o-bromo phenol solution (3), controlling the stirring speed at 130-150rpm, 0.26mol cuprous chloride was added, 310ml potassium chloride solution, controlling the temperature of the solution at 10-15 C, reacted for 7-9h, the temperature of the solution is reduced to 5-8 C, by adding ammonium nitrate solution, the pH was adjusted to 6-7, extracted with dimethylsulfoxide 5-7 times, the combined organic layers was washed with cyclohexanol solution, dehydrated with a dehydrating agent, dimethylsulfoxide was distilled off under vacuum distillion, the residue was added to N-dimethylformamide solution, precipitated solid was filtered, recrystallized from acetamide solution, got crystals 2-(1H-1-tetrazolyl) acetic acid.
机译:#$%^&* AU2016102314A420170223.pdf #####抽象头孢唑醇药物中间体2-(1H-1-4咪唑基)乙酸合成方法,包括以下步骤:(I)反应容器加入0.51mol 2-(5-硝基-1H-1-四唑基)乙酸(2),0.56-0.59mol邻溴苯酚溶液(3),控制搅拌速度在130-150rpm下,加入0.26mol氯化亚铜,310ml钾氯化物溶液,将溶液温度控制在10-15 C,反应7-9h,溶液温度降至5-8 C,加入硝酸铵溶液,调节pH至6-7,萃取用二甲亚砜5-7次,合并有机层用环己醇溶液洗涤,用脱水剂脱水,真空蒸馏除去二甲亚砜,残留物将其加入到N-二甲基甲酰胺溶液中,沉淀出的固体为过滤,从乙酰胺溶液中重结晶,得到晶体2-(1H-1-四唑基)乙酸。

著录项

  • 公开/公告号AU2016102314A4

    专利类型

  • 公开/公告日2017-02-23

    原文格式PDF

  • 申请/专利权人 XIAMEN KAI ER LI INFORMATION TECHNOLOGY CO. LTD;

    申请/专利号AU20160102314

  • 发明设计人 GUAN GENAN;

    申请日2016-12-25

  • 分类号C07D257/04;

  • 国家 AU

  • 入库时间 2022-08-21 13:32:35

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